Carbamoylation Using Organic Azides and Phosphine

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Solution Overview

Problem

Existing methods for carbamoylation of amines, mercaptanes, thiophenols, and phenols using organic azides require expensive transition metal complexes and hazardous gases like carbon monoxide, necessitating specialized equipment and complex procedures.

Innovation Solution

A method employing an organic azide, trivalent phosphorous compounds like triphenylphosphine, and an aqueous trialkylammonium hydrogen carbonate buffer in a simple, closed vessel setup, avoiding the need for expensive catalysts and toxic gases, to generate isocyanates for urea, thiocarbamate, and carbamate derivatives.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If transition metal complexes and carbon monoxide gas are used for carbamoylation, then the reaction can proceed, but the equipment complexity and safety hazards increase significantly

Engineering Contradiction:
Improvereaction reliabilityVSAvoidequipment complexity
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The patent extracts and eliminates the hazardous carbon monoxide gas and expensive transition metal complexes from the reaction system. Instead, it uses benign carbon dioxide and inexpensive phosphine catalysts, thereby removing the need for specialized high-pressure equipment while maintaining reaction reliability

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent replaces expensive transition metal complexes with inexpensive phosphine compounds that can be used in simple closed vessels. The method uses readily available carbon dioxide instead of costly carbon monoxide, making the process accessible to ordinary laboratories without specialized equipment

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

2Productivity

If carbon monoxide gas is used for carbamoylation, then the reaction efficiency is maintained, but the safety hazards and operational complexity increase

Engineering Contradiction:
Improvereaction efficiencyVSAvoidsafety hazards
Core Design Contradiction:
ProductivityVSObject-affected harmful factors

Solution Approach 1:

The patent converts the typically harmful carbon monoxide gas into a beneficial process by using harmless carbon dioxide instead. This substitution eliminates safety hazards while maintaining reaction efficiency, as carbon dioxide is naturally abundant and non-toxic

Inventive Principle:
Principle #22Blessing in disguise (Convert harm into benefit)

Solution Approach 2:

The patent changes the physical and chemical parameters of the carbon source from gaseous carbon monoxide under high pressure to gaseous or soluble carbon dioxide at ambient conditions. This parameter change eliminates safety hazards while preserving the carbamoylation reaction efficiency

Inventive Principle:
Principle #35Parameter changes

3Reliability

If specialized equipment and transition metal complexes are used, then the carbamoylation reaction can be performed, but the cost and accessibility decrease

Engineering Contradiction:
Improvereaction reliabilityVSAvoidprocess accessibility
Core Design Contradiction:
ReliabilityVSEase of manufacture

Solution Approach 1:

The patent employs inexpensive phosphine catalysts and readily available carbon dioxide, eliminating the need for expensive transition metal complexes and specialized equipment. This makes the carbamoylation process accessible to any chemical laboratory while maintaining reliable reaction outcomes

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

Solution Approach 2:

The patent creates a universal carbamoylation method that can be performed in simple closed vessels using common laboratory equipment. The use of phosphine catalysts and carbon dioxide makes the process universally applicable across different laboratories without requiring specialized setups

Inventive Principle:
Principle #6Universality (Multi-functionality)

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

This method simplifies the carbamoylation process, making it accessible in any chemical laboratory, achieving high-efficiency conjugation and stability in products suitable for nucleoside synthesis, oligonucleotide modification, and various industrial applications without the need for specialized equipment or hazardous reagents.

Implementation Method 1

reacting a compound of formula R-N3 with triphenylphosphine in the presence of an aqueous solution of hydrogen carbonate ions to obtain an isocyanate

Methodology Applied
Scientific EffectReduction: Reduction

Implementation Method 2

reacting the isocyanate with a compound of formula R'-XH to obtain a compound of formula IV

Methodology Applied
Scientific EffectChemical Bonding: Chemical Bonding

Data Source

PatentEP2076488B1Carbamoylation of amines, thiophenols, mercaptanes and phenols employing organic azides
Publication Date: 2016.05.11 METKINEN CHEM
  • EP2076488B1 patent drawingFigure 1~2
  • EP2076488B1 patent drawingFigure 3~5
  • EP2076488B1 patent drawingFigure 6

AI summary

The present invention relates to carbamoylation of amines, mercaptanes, thiophenols and phenols employing organic azides. More specifically, the invention relates to a method for generating urea derivatives, thiocarbamate derivatives and carbamate derivatives, and is based on the intermediate formation of isocyanate, starting from an organic azide. The reaction as described is useful in applications for modified nucleoside synthesis, oligonucleotide synthesis, as well as modification, labeling and conjugation of polymers and biomolecules.